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Acetaldehyde → alpha-Methyl-N-phenyl-1H-benzotriazole-1-methanamine

HRID 585362
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HRID 585362 반응식
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.[NH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH:17](=O)[CH3:18]>C(OCC)C>[CH3:17][CH:18]([N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1)[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
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참가 물질

5

반응물 3

HCID 177AcetaldehydeHCID 6115AnilineHCID 178418385HCID 178418385, 화합물

생성물 1

HCID 3451461alpha-Methyl-N-phenyl-1H-benzotriazole-1-methanamine수율 869.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Benzotriazole (5.0 g, 4.20 mmol) and aniline (3.91 g, 4.20 mmol) were dissolved in diethyl ether (85 ml), and acetaldehyde (2.03 g, 4.62 mmol) was added dropwise thereto on ice. The reaction mixture was stirred at room temperature for 15 minutes and then allowed to stand overnight at −20° C. The crystallized product was collected by filtration, washed with diethyl ether and then dried to give α-methyl-N-phenyl-1H-benzotriazole-1-methanamine (8.7 g) as a white crystal. The resulting α-methyl-N-phenyl-1H-benzotriazole-1-methanamine (2.86 g, 12 mmol) and vinylphthalimide (2860 mg, 12.0 mmol) were suspended in chloroform (10 ml), to which p-toluenesulfonic acid monohydrate (190 mg, 1.0 mmol) was then added and stirred at room temperature for 10 hours. After addition of water, the reaction mixture was extracted with chloroform. The organic layer was washed with saturated aqueous sodium carbonate and water, and then concentrated. The residue was applied to silica gel column chromatography to give the titled compound (1.03 g, yield over 2 steps: 25%) as a white crystal.

후처리

  1. waitto stand overnight at −20° C
  2. filtrationThe crystallized product was collected by filtration
  3. washwashed with diethyl ether
  4. customdried

출처 및 근거

ORD 기록
ord-28cc3cd76dec4c5c8638bc4e286e3925
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06930104B2

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